EP0835609A1 - Entmineralisierung von Käserei-Süssmolke - Google Patents

Entmineralisierung von Käserei-Süssmolke Download PDF

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Publication number
EP0835609A1
EP0835609A1 EP97202935A EP97202935A EP0835609A1 EP 0835609 A1 EP0835609 A1 EP 0835609A1 EP 97202935 A EP97202935 A EP 97202935A EP 97202935 A EP97202935 A EP 97202935A EP 0835609 A1 EP0835609 A1 EP 0835609A1
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EP
European Patent Office
Prior art keywords
compartments
resin
dilution
demineralization
concentration
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP97202935A
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English (en)
French (fr)
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EP0835609B1 (de
Inventor
Rafael Berrocal
Michel Chaveron
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Societe des Produits Nestle SA
Nestle SA
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Societe des Produits Nestle SA
Nestle SA
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Priority to EP19970202935 priority Critical patent/EP0835609B1/de
Publication of EP0835609A1 publication Critical patent/EP0835609A1/de
Application granted granted Critical
Publication of EP0835609B1 publication Critical patent/EP0835609B1/de
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
    • B01D61/44—Ion-selective electrodialysis
    • B01D61/46—Apparatus therefor
    • B01D61/48—Apparatus therefor having one or more compartments filled with ion-exchange material, e.g. electrodeionisation
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00—Milk preparations; Milk powder or milk powder preparations
    • A23C9/14—Milk preparations; Milk powder or milk powder preparations in which the chemical composition of the milk is modified by non-chemical treatment
    • A23C9/144—Milk preparations; Milk powder or milk powder preparations in which the chemical composition of the milk is modified by non-chemical treatment by electrical means, e.g. electrodialysis
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00—Milk preparations; Milk powder or milk powder preparations
    • A23C9/14—Milk preparations; Milk powder or milk powder preparations in which the chemical composition of the milk is modified by non-chemical treatment
    • A23C9/146—Milk preparations; Milk powder or milk powder preparations in which the chemical composition of the milk is modified by non-chemical treatment by ion-exchange

Definitions

  • the invention relates to the field of demineralization of sweet whey from cheese dairy.
  • Demineralized whey liquid or powder
  • Demineralized whey is the main component of infant and dietetic products, in particular milks suitable for breast milk.
  • Demineralized whey also has d other applications, for example as a substitute for skimmed milk in confectionery-chocolate or in the manufacture of reconstituted milks.
  • the most effective known methods for demineralizing whey are: electrodialysis and exchange of ions, which are applied separately or in combination.
  • electrodialysis the ionized salts in solution in the whey migrate under the effect of an electric field through membranes selectively permeable to cations and anions and are eliminated in the form of brine.
  • L exchange of ions we use l ionic balance between a resin as a solid phase and the whey to be demineralized as a liquid phase, the ions being adsorbed on the resin of the same kind during the saturation phase, then the resins then regenerated.
  • L electrodionization making the object for example from US-A-4632745 or from US-A-5120416, continuously performs deionization in the treatment of water by combining l electrodialysis and exchange of ions in a single module, which has the advantages of low consumption d water and d energy and eliminates the need to chemically regenerate resins.
  • This technique consists in circulating l water to be demineralized through a set of parallel cells delimited by cationic and anionic semipermeable membranes and containing a mixture of resin beads, called dilution compartments, these dilution compartments being separated from each other and their whole being separated from the outside by spacers, forming so-called concentration compartments, delimited by anionic and cationic semi-permeable membranes, the whole being placed between a cathode compartment and an anode compartment under tension.
  • concentration compartments delimited by anionic and cationic semi-permeable membranes
  • the resin beads loaded with adsorbed ions maintain satisfactory electrical conductivity in the dilution compartments throughout the demineralization process. In addition, there is no it is not necessary to regenerate them, since the sites saturated in cations and in anions are exchanged progressively against ions H + and OH - under l electric field effect.
  • the resin beads are fixedly incorporated in the dilution compartments while in the process according to US-A-5120416, the beads are mobile and it is possible to introduce them into the compartments dilution and to extract them by circulation in the form of a suspension.
  • the resins come in a mixed bed of beads of strong cationic and strong anionic type.
  • L invention relates to a process for demineralizing sweet whey from a cheese dairy, characterized in that the a mild, more or less concentrated cheese whey is electrodionized in an apparatus, the dilution compartments or the concentration and dilution compartments containing resin beads consisting of cationic resin alone or d a mixture of cationic resin and weak anionic resin and that the pH of the concentration compartments is adjusted to a value less than 5.
  • soft cheese whey is the liquid obtained after coagulation of casein by rennet during the manufacture of cheese.
  • the raw material can be raw, more or less concentrated or even reconstituted in an aqueous medium from powder.
  • any material usually used in resin can be used as resin. exchange of ions, for example macroréticulé, in the form of gel or macroporous, provided that this material has the rigidity compatible with confinement in cells and does not fix the proteins by absorption or adsorption.
  • a mixture of cationic resin and weak anionic queen can be used.
  • the cationic resin a weak or strong cationic resin or a mixture of these resins can be used.
  • a weak cationic resin generally has a high capacity for relatively large adsorption and swelling.
  • a strong cationic resin has a capacity of weaker adsorption and limited swelling.
  • the electrodionization with strong cationic resin beads alone in the dilution compartments we have found that the demineralization of the anions that l we want to eliminate, essentially Cl - and citrates, as well as that of the cations, essentially K + , Na + , Ca ++ and Mg ++ , s performed satisfactorily without significant protein loss, with l advantage of better microbiological quality at temperature d about 30 ° C, due to the work leading to a low final pH, of the order of 3 to 4. Furthermore, the non-protein nitrogen decreased, which increased the content of true proteins, sought in particular in infant products and at the same time modified the aminogram of the product.
  • the strong cationic resin is preferably in H + form and the weak anionic resin preferably in OH - form.
  • the pH of the substrate When you want a deep de-anionization, it is preferable to increase the pH of the substrate, either at the start of the demineralization process, or when the demineralization rate has reached around 70%, to a value of around 7.5-8, by alkalinization, for example by a strong base such as KOH.
  • alkalinization for example by a strong base such as KOH.
  • Ca hydroxide and if necessary heat for example to about 45 ° C / 20 min., then eliminate the precipitate to form.
  • Another variant of this de-anionization consists in passing the substrate, for example about 80% demineralized, through a column of weak anionic resin.
  • the process according to l invention can be implemented in continuous mode, in which case the substrate d a part can be directed to the dilution compartment of the module, then evacuated from this compartment as and when in the form of demineralized product and the washing flow can also be directed to the concentration compartment and, depending on the version, the brine or the dilute hydrochloric acid be evacuated as and when.
  • the substrate in batch or batch mode, can be recirculated in a loop through the dilution compartment and the brine recirculated in a loop through the concentration compartment, up to that l the desired demineralization rate is reached.
  • the reactant obtained can be neutralized if necessary by adding an alkali, preferably of food grade, then dried, for example by spraying in a drying tower.
  • the product obtained by implementing the process according to l invention that either liquid or powder, can be used as ingredient in the manufacture of a food intended for human or animal food.
  • lactoproteins c ie a partly delactose product containing in particular approximately 30 to 40% by weight of proteins and approximately 45 to 55% by weight of lactose or a demineralized whey product containing in particular approximately 9 to 15% by weight of proteins and approximately 75 to 85 % by weight of lactose.
  • It can be used as a substitute for milk or whey as an ingredient the manufacture of confectionery-chocolate or frozen confectionery products and in particular as a whey replacer in the manufacture of infant products, in particular milk adapted for breast milk.
  • Figure 1 schematically shows a simplified apparatus d electrodionization.
  • a single sequence of alternating cells is represented therein whereas in reality a module comprises several sequences of alternating cells arranged in parallel.
  • module 1 alternately comprises polymer membranes semi-permeable 2a, 2b, permeable to cations and impermeable to anions, negatively charged, for example by sulfonic groups and 3a, 3b, permeable to anions and impermeable to cations, positively charged, by example carrying quaternary ammonium groups between electrodes, a anode 4 and a cathode 5.
  • the membranes 2b and 3a delimit a cell filled with resin beads, by strong cationic 6 and weak anionic example 7, in mixed beds, constituting a dilution compartment 8 surrounded by two delimited spacers respectively by membranes 2a, 3a and 2b, 3b, filled with resin ball or resin-free, forming the concentration compartments 9a, 9b.
  • the anode 10 and cathode 11 compartments surround the compartments of concentration 9a, 9b located at the ends of the module.
  • the flow of substrate to be demineralized 12 crosses the dilution compartment 8 in which it is freed from its cations such as C + adsorbed by the strong cationic resin and from its anions such as A - adsorbed by the weak anionic resin.
  • Demineralization takes place discontinuously, by charges, c i.e. by recirculating the substrate through the module until until the entire volume of the charge has reached the target conductivity.
  • the conductivity of the concentration compartment (providing the ion collection flux) is maintained at a value ⁇ 30 mS (milli Siemens) by replacing half of the solution with l distilled water when this conductivity value is reached.
  • c is to say when the demineralization rate chosen a priori, which n is not the maximum possible demineralization rate, is reached, the current is cut off, the total volume of demineralized reactant is collected, that is the permeate, it is weighed and dried by lyophilization.
  • the brine of the concentration or retentate compartment and with the solutions of the compartments of electrodes.
  • the module is rinsed several times with distilled water or, if necessary, washed with a solution containing 2.5% NaCl / 1% NaOH or with a solution of 5% NaCl / 1% Na percarbonate, rinsed with distilled water and keep it filled with water between charges.
  • Example 1 2 Resin type, strong% cation / weak anionic mixture% HP111 (form H + ) / HP661 (form OH - ), Rohm & Haas, 40/60 HP111 (form H + ) / HP661 (form OH - ), Rohm & Haas, 40/60, sweet whey, preconcentrated by evaporation Mild whey, material, dry (%) 6.7 18.2 Flow (l / min) 0.7 0.7 Duration of treatment (min) 35 94 final pH 4.1 5.35 Demineralization rate (%) 91.76 87.13 TN lost in% of l initial 11.51 8.96 True protein lost in% of l initial 6.39 5.24
  • Example 4 5 Mild whey, dry matter (%) 6.7 6.7 Duration of treatment (min) 28 25 Flow (l / min) 0.7 1.4 final pH 3.06 3.69 Demineralization rate (%) 95.02 83.88 TN lost in% of l initial 8.45 2.14 True protein lost in% of l initial 1.27 - 2.27 Legend: - means that part of the non-protein nitrogen disappears from the substrate during treatment, which explains a negative loss and therefore a gain in true protein.
  • Example 2 We proceed as in Example 2 to demineralize a sweet whey preconcentrated cheese, but filling the dilution compartment with a mixture of 40/60% strong cationic resin, HP 111 (form H +) / weak anionic resin, HP 661 (OH- form), Rohm & Haas and leaving empties the concentration compartment.
  • the pH in the concentration compartment has increased to a value close to 5, and there is a decrease regular flow and increased pressure in this compartment.
  • Example 2 We proceed as in Example 2 to demineralize a sweet whey preconcentrated cheese, but filling the dilution compartment with a mixture of 40/60% strong cationic resin, HP 111 (form H +) / weak anionic resin, HP 661 (OH- form), Rohm & Haas and the concentration compartment with strong cationic resin, HP 111 (form H +). Under these conditions, it is the strong resin which maintains the pH in the acidic domain.
  • the conductivity in the electrode compartments is maintained at 5-20 mS by continuously adding an aqueous sulfuric acid solution.
  • Example 6 The procedure is as in Example 6, apart from the fact that, once the level of 75% demineralization has been reached, the pH of the substrate entering the apparatus is adjusted to 7.5-8 by addition of an aqueous solution of KOH, and the pH is maintained at this value up to a level of demineralization of 90%. There is thus obtained a substantial reduction in the amount of anions present in the final liquid whey, in comparison with what is obtained without prior adjustment of the pH, as shown in Table 4 below.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Water Supply & Treatment (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Urology & Nephrology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dairy Products (AREA)
EP19970202935 1996-10-09 1997-09-25 Entmineralisierung von Käserei-Süssmolke Expired - Lifetime EP0835609B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP19970202935 EP0835609B1 (de) 1996-10-09 1997-09-25 Entmineralisierung von Käserei-Süssmolke

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP96202810 1996-10-09
EP96202810 1996-10-09
EP19970202935 EP0835609B1 (de) 1996-10-09 1997-09-25 Entmineralisierung von Käserei-Süssmolke

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EP0835609A1 true EP0835609A1 (de) 1998-04-15
EP0835609B1 EP0835609B1 (de) 2004-06-23

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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1193630A (fr) * 1955-12-08 1959-11-04 Procédé et dispositif pour enlever des sels de liquides qui en contiennent
US3645884A (en) * 1969-07-10 1972-02-29 Edwin R Gilliland Electrolytic ion exchange apparatus
FR2391653A1 (fr) * 1977-05-23 1978-12-22 Nestle Sa Soc Ass Tech Prod Procede de traitement du lactoserum
JPS5811004A (ja) * 1981-07-15 1983-01-21 Tokuyama Soda Co Ltd 電解質水溶液の脱塩方法
EP0170895A2 (de) * 1984-07-09 1986-02-12 Millipore Corporation Vorrichtung und Verfahren zur elektrischen Entionisierung
EP0417506A1 (de) * 1989-09-08 1991-03-20 Millipore Corporation Behandlungsverfahren durch elektrische Entionisierung und UV-Licht zur Reinigung von Wasser
US5066375A (en) * 1990-03-19 1991-11-19 Ionics, Incorporated Introducing and removing ion-exchange and other particulates from an assembled electrodeionization stack
US5084285A (en) * 1989-06-01 1992-01-28 Snow Brand Milk Products, Co., Ltd. Desalting process of milk
US5120416A (en) * 1990-03-19 1992-06-09 Ionics, Incorporated Introducing and removing ion-exchange and other particulates from an assembled electrodeionization stack
WO1995029005A1 (en) * 1994-04-25 1995-11-02 Ionics, Incorporated Improvements in electrodialysis including filled cell electrodialysis (electrodeionization)

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1193630A (fr) * 1955-12-08 1959-11-04 Procédé et dispositif pour enlever des sels de liquides qui en contiennent
US3645884A (en) * 1969-07-10 1972-02-29 Edwin R Gilliland Electrolytic ion exchange apparatus
FR2391653A1 (fr) * 1977-05-23 1978-12-22 Nestle Sa Soc Ass Tech Prod Procede de traitement du lactoserum
JPS5811004A (ja) * 1981-07-15 1983-01-21 Tokuyama Soda Co Ltd 電解質水溶液の脱塩方法
EP0170895A2 (de) * 1984-07-09 1986-02-12 Millipore Corporation Vorrichtung und Verfahren zur elektrischen Entionisierung
US4632745A (en) * 1984-07-09 1986-12-30 Millipore Corporation Electrodeionization apparatus
US4632745B1 (en) * 1984-07-09 1994-06-28 Millipore Invest Holdings Electrodeionization apparatus
US5084285A (en) * 1989-06-01 1992-01-28 Snow Brand Milk Products, Co., Ltd. Desalting process of milk
EP0417506A1 (de) * 1989-09-08 1991-03-20 Millipore Corporation Behandlungsverfahren durch elektrische Entionisierung und UV-Licht zur Reinigung von Wasser
US5066375A (en) * 1990-03-19 1991-11-19 Ionics, Incorporated Introducing and removing ion-exchange and other particulates from an assembled electrodeionization stack
US5120416A (en) * 1990-03-19 1992-06-09 Ionics, Incorporated Introducing and removing ion-exchange and other particulates from an assembled electrodeionization stack
WO1995029005A1 (en) * 1994-04-25 1995-11-02 Ionics, Incorporated Improvements in electrodialysis including filled cell electrodialysis (electrodeionization)

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
PATENT ABSTRACTS OF JAPAN vol. 007, no. 083 (C - 160) 6 April 1983 (1983-04-06) *
R. DELANAY: "Demineralisation of whey", AUSTRALIAN JOURNAL OF DAIRY TECHNOLOGY, vol. 3, no. 1, 1976, HIGHETT VIC AU, pages 12 - 17, XP002027447 *

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